CN112852412B - Method for rapidly synthesizing high-fluorescence sulfur quantum dots - Google Patents

Method for rapidly synthesizing high-fluorescence sulfur quantum dots Download PDF

Info

Publication number
CN112852412B
CN112852412B CN202110066431.8A CN202110066431A CN112852412B CN 112852412 B CN112852412 B CN 112852412B CN 202110066431 A CN202110066431 A CN 202110066431A CN 112852412 B CN112852412 B CN 112852412B
Authority
CN
China
Prior art keywords
sulfur
quantum dots
sulfur quantum
sulfide
sulfur powder
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202110066431.8A
Other languages
Chinese (zh)
Other versions
CN112852412A (en
Inventor
蓝敏焕
李香草
赵少静
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Central South University
Original Assignee
Central South University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Central South University filed Critical Central South University
Priority to CN202110066431.8A priority Critical patent/CN112852412B/en
Publication of CN112852412A publication Critical patent/CN112852412A/en
Application granted granted Critical
Publication of CN112852412B publication Critical patent/CN112852412B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/56—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing sulfur
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K38/00—Medicinal preparations containing peptides
    • A61K38/16—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof
    • A61K38/43—Enzymes; Proenzymes; Derivatives thereof
    • A61K38/44—Oxidoreductases (1)
    • A61K38/443—Oxidoreductases (1) acting on CH-OH groups as donors, e.g. glucose oxidase, lactate dehydrogenase (1.1)
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K41/00—Medicinal preparations obtained by treating materials with wave energy or particle radiation ; Therapies using these preparations
    • A61K41/0052—Thermotherapy; Hyperthermia; Magnetic induction; Induction heating therapy
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/50—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient the non-active ingredient being chemically bound to the active ingredient, e.g. polymer-drug conjugates
    • A61K47/51—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient the non-active ingredient being chemically bound to the active ingredient, e.g. polymer-drug conjugates the non-active ingredient being a modifying agent
    • A61K47/54—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient the non-active ingredient being chemically bound to the active ingredient, e.g. polymer-drug conjugates the non-active ingredient being a modifying agent the modifying agent being an organic compound
    • A61K47/55—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient the non-active ingredient being chemically bound to the active ingredient, e.g. polymer-drug conjugates the non-active ingredient being a modifying agent the modifying agent being an organic compound the modifying agent being also a pharmacologically or therapeutically active agent, i.e. the entire conjugate being a codrug, i.e. a dimer, oligomer or polymer of pharmacologically or therapeutically active compounds
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/50—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient the non-active ingredient being chemically bound to the active ingredient, e.g. polymer-drug conjugates
    • A61K47/51—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient the non-active ingredient being chemically bound to the active ingredient, e.g. polymer-drug conjugates the non-active ingredient being a modifying agent
    • A61K47/62—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient the non-active ingredient being chemically bound to the active ingredient, e.g. polymer-drug conjugates the non-active ingredient being a modifying agent the modifying agent being a protein, peptide or polyamino acid
    • A61K47/64—Drug-peptide, drug-protein or drug-polyamino acid conjugates, i.e. the modifying agent being a peptide, protein or polyamino acid which is covalently bonded or complexed to a therapeutically active agent
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K49/00—Preparations for testing in vivo
    • A61K49/001—Preparation for luminescence or biological staining
    • A61K49/0063—Preparation for luminescence or biological staining characterised by a special physical or galenical form, e.g. emulsions, microspheres
    • A61K49/0065—Preparation for luminescence or biological staining characterised by a special physical or galenical form, e.g. emulsions, microspheres the luminescent/fluorescent agent having itself a special physical form, e.g. gold nanoparticle
    • A61K49/0067—Preparation for luminescence or biological staining characterised by a special physical or galenical form, e.g. emulsions, microspheres the luminescent/fluorescent agent having itself a special physical form, e.g. gold nanoparticle quantum dots, fluorescent nanocrystals
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P35/00—Antineoplastic agents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B17/00—Sulfur; Compounds thereof
    • C01B17/02—Preparation of sulfur; Purification
    • C01B17/027—Recovery of sulfur from material containing elemental sulfur, e.g. luxmasses or sulfur containing ores; Purification of the recovered sulfur
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B17/00—Sulfur; Compounds thereof
    • C01B17/02—Preparation of sulfur; Purification
    • C01B17/06—Preparation of sulfur; Purification from non-gaseous sulfides or materials containing such sulfides, e.g. ores
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
    • C09K11/025—Use of particular materials as binders, particle coatings or suspension media therefor non-luminescent particle coatings or suspension media
    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12Y—ENZYMES
    • C12Y101/00—Oxidoreductases acting on the CH-OH group of donors (1.1)
    • C12Y101/03—Oxidoreductases acting on the CH-OH group of donors (1.1) with a oxygen as acceptor (1.1.3)
    • C12Y101/03004—Glucose oxidase (1.1.3.4)
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/64—Fluorescence; Phosphorescence
    • G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
    • G01N21/643—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes" non-biological material
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/64—Fluorescence; Phosphorescence
    • G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
    • G01N2021/6432—Quenching

Landscapes

  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Organic Chemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Bioinformatics & Cheminformatics (AREA)
  • Veterinary Medicine (AREA)
  • Public Health (AREA)
  • Animal Behavior & Ethology (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Medicinal Chemistry (AREA)
  • Epidemiology (AREA)
  • Nanotechnology (AREA)
  • Physics & Mathematics (AREA)
  • Inorganic Chemistry (AREA)
  • Immunology (AREA)
  • Materials Engineering (AREA)
  • Proteomics, Peptides & Aminoacids (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Geology (AREA)
  • Optics & Photonics (AREA)
  • General Physics & Mathematics (AREA)
  • Biochemistry (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Molecular Biology (AREA)
  • Biomedical Technology (AREA)
  • Gastroenterology & Hepatology (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • General Engineering & Computer Science (AREA)
  • Genetics & Genomics (AREA)
  • Wood Science & Technology (AREA)
  • Zoology (AREA)
  • Biophysics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Analytical Chemistry (AREA)
  • Pathology (AREA)

Abstract

The invention provides a method for rapidly synthesizing a strong fluorescent sulfur quantum dot. The preparation method comprises the following steps: adding sulfur powder and metal sulfide into a dispersion system to obtain dispersion liquid; the dispersion system comprises protein and water; introducing oxidizing gas into the system, and stirring and reacting under a heating condition; and after the reaction is finished, cooling to room temperature, and performing purification treatment through centrifugation, filtration and dialysis to obtain the sulfur quantum dots. The method for preparing the sulfur quantum dots by oxidizing the oxidizing gas has the advantages of short reaction time, high fluorescence quantum yield, rich surface functional groups, uniform particle size distribution, good water solubility and biocompatibility, high stability and the like, and has great application potential and significance in a plurality of fields.

Description

Method for rapidly synthesizing high-fluorescence sulfur quantum dots
Technical Field
The invention belongs to the technical field of nano materials, and relates to a method for synthesizing a sulfur quantum dot with strong fluorescence prepared by oxidizing gas and passivating protein.
Background
The sulfur quantum dots are dispersed sphere-like fluorescent sulfur nanoparticles with the size at the nanometer level. The sulfur quantum dots prepared from the sulfur powder and the protein show good chemiluminescence characteristics such as high fluorescence intensity, high light stability, photobleaching resistance, low toxicity and the like, and can be used in various fields such as detection, catalysis, imaging, treatment and the like.
At present, cheap and easily-obtained green and environment-friendly synthetic raw materials and a simple and rapid preparation method are adopted, and the high quantum yield and the red/near-infrared luminescent sulfur quantum dots are required to be further developed and researched. However, to date, there has been only a small amount of research on sulfur quantum dots. Currently, sulfur quantum dots are mainly synthesized by technologies such as an oil-water microemulsion technology, a cystine modified nano sulfur formula and a liquid synthesis method. Compared with the sulfur quantum dots synthesized by the prior art, the quantum yield is lower, and the operation steps of the synthetic reaction are relatively complex and tedious. In recent years, blue light sulfur quantum dots with quantum yield of 3.8% are obtained by simply placing sulfur powder in an alkaline solution for heating and stirring. Although the method can improve the quantum yield of the sulfur quantum dots, the method takes longer time, and the quantum yield still needs to be further improved to be more widely applied.
In view of the problems of low quantum yield, complex preparation and long reaction time of the existing preparation method of the sulfur quantum dots; therefore, a method for rapidly synthesizing the high-fluorescence sulfur quantum dots is urgently needed.
Disclosure of Invention
Based on the defects in the prior art, the invention aims to provide a preparation method and application of sulfur quantum dots, the preparation method has the advantages of easily available raw materials, low price and simple preparation method, and can solve the problems of long time consumption, complex operation steps, low fluorescence quantum yield and the like in the prior art for preparing the sulfur quantum dots; the invention has the advantages of green economy, rapid preparation, convenient operation, high fluorescence quantum yield and wide application potential.
The purpose of the invention is realized by the following technical means:
in one aspect, the invention provides a preparation method of a sulfur quantum dot, which comprises the following steps:
step one, adding sulfur powder and metal sulfide into a dispersion system to obtain dispersion liquid; the dispersion system comprises protein and water;
transferring the dispersion liquid into a round-bottom flask, introducing oxidizing gas, and reacting for a period of time under heating and stirring;
and step three, cooling to room temperature after the reaction is finished, and carrying out purification treatment through centrifugation, filtration and dialysis to obtain the sulfur quantum dots.
In the preparation method of the sulfur quantum dots, the metal sulfide and the protein are added to synergistically enhance the fluorescence intensity of the sulfur quantum dots and influence the emission wavelength, so that the complicated steps are reduced, and the reaction time is shortened; the raw materials adopted by the invention are green, safe and easily available, the reaction conditions are mild, the requirements on equipment are low, and the prepared sulfur quantum dots have good water solubility, good dispersibility, stable performance and high fluorescence quantum yield.
In the above method, preferably, the mass of the sodium sulfide is 5 to 10 g; further preferably, the mass of the sodium sulfide is 5 g.
In the above method, preferably, the sulfur includes one or more of sublimed sulfur powder, elemental sulfur, sulfur blocks, sulfur granules, and sulfur powder; further preferably, the sulfur is sublimed sulfur powder.
In the above method, the BSA has a mass of 0.05 to 0.1 g; further preferably, the BSA has a mass of 0.1 g.
In the above method, preferably, the ratio of the amounts of the sulfur powder, the sodium sulfide, the BSA, and the water is (0.05 to 1 g): (5-10 g): (0.05-0.10 g): (10-60 mL).
In the above method, preferably, the flow rate of the ozone is 1 to 100 mL/min; further preferably, the flow rate of the ozone is 50 mL/min.
In the above method, preferably, the reaction temperature is 25 to 150 ℃; further preferably, the reaction temperature is 90 ℃.
In the above method, preferably, the prepared sulfur quantum dot further comprises a purification step, specifically:
and centrifuging the sulfur quantum dots, and filtering the obtained supernatant by using a microporous filter membrane or dialyzing by using a dialysis bag to remove impurities to obtain pure sulfur quantum dots.
In the method, preferably, the rotation speed of the sulfur quantum dots for centrifugation is 100-2000 rpm, and the centrifugation time is 0.1-10 h; further preferably, the centrifuge rotation speed is 2000rpm and the centrifugation time is 30 min.
In the above method, preferably, the pore diameter of the microporous filter membrane is 0.22 to 0.45 μm; further preferably, the pore size of the microfiltration membrane is 0.22 μm.
In the method, a dialysis bag with a molecular interception amount of 500-5000 Da is preferably adopted for dialysis; the dialysis time is 24-72 h; further preferably, a dialysis bag with the molecular interception amount of 500-1000 Da is adopted for dialysis; the dialysis time was 24 h.
The invention has the beneficial effects that:
(1) in the preparation method of the sulfur quantum dot, the dispersant BSA is added and the O is introduced3The oxidation can accelerate the reaction time, synergistically enhance the fluorescence intensity of the sulfur spot and change the emission wavelength, and BSA and O are creatively added3The oxidation can synergistically promote the reaction to be carried out more efficiently, so that the complicated steps are reduced, and the reaction time is shortened; the raw materials adopted by the invention are green, safe and easily available, the reaction conditions are mild, the requirements on equipment are low, and the prepared sulfur quantum dots have high yield, rich surface functional groups, small size, uniform particle size distribution, good water solubility and good light stability; the fluorescent material has wide application prospect in the fields of analysis and detection, photocatalysis and disease treatment as a luminescent material.
Drawings
FIG. 1 is a schematic diagram of a transmission electron microscope for synthesizing fluorescent sulfur quantum dots.
FIG. 2 shows the emission intensity and color of sulfur quantum dots irradiated by an ultraviolet lamp at different reaction times.
FIG. 3 wavelength dependent spectral response of sulfur quantum dots at 1.5 and 5 h.
FIG. 4 wavelength dependent spectral response of the sulfur quantum dots at 7 and 10 h.
FIG. 5 xenon lamp irradiation (1W/cm)-2) And testing the light stability of the sulfur quantum dots and the fluorescein sodium.
FIG. 6 shows the sulfur quantum dots to metal ions Hg2+Titration and interference rejection diagrams.
The specific implementation mode is as follows:
the embodiment of the invention provides a method for rapidly synthesizing high-fluorescence sulfur quantum dots, which comprises the following steps:
example 1
At room temperature, 1g of sulfur powder and 5g of Na2S and 0.1g BSA,50mL H2Placing O in a round-bottom flask, and carrying out ultrasonic treatment for 10 min;
(2) setting the reaction temperature at 90 ℃ and the reaction time at 5h, and naturally cooling to room temperature after the reaction is finished.
(3) Centrifugation was performed, and the supernatant was taken. In order to obtain the pure sulfur quantum dots with uniform size distribution and without impurities such as unreacted raw materials and the like, the centrifuged supernatant is filtered for three times through a microporous filter membrane or placed in a dialysis bag for dialysis. And (3) placing the filtrate or the dialysate into a vacuum drying oven for heating, concentrating and drying, wherein the obtained solid sulfur quantum dots can be dissolved in other solvents such as water and the like so as to meet the requirements of different application aspects.
FIG. 1 is a TEM micrograph of the sulfur quantum dots prepared in example 1. As can be seen from figure 1, the sulfur quantum dots obtained by ozone oxidation have small particle size of 3nm and uniform distribution.
FIG. 2 is a graph of the emission of ozone-oxidized sulfur quantum dots under an ultraviolet lamp, as provided in example 1 of the present invention. It can be seen from the figure that the fluorescence intensity of the sulfur quantum dots is stronger and stronger, the fluorescence color is changed from blue to green, and the fluorescence is strongest at the time of 5 h.
FIGS. 3a,3b and FIGS. 4a,4b are fluorescence spectra of the ozonized sulfur quantum dots provided in example 1 of the present invention with reaction times of 1.5, 5h, 7h and 10 h. The spectrogram shows that the sulfur quantum dot has strong fluorescence intensity when the reaction time is 5 hours, the quantum yield is 25 percent, the wavelength is red-shifted, and the emission wavelength is 520 nm.
FIG. 5 is a photo-stability test of the sulfur quantum dots prepared by the invention, and the sulfur quantum dots have good photo-stability as can be seen by comparing with sodium fluorescein.
The sulfur quantum dots obtained by the preparation method and conditions are used forAnalysis and detection of heavy metal ions Hg2+As the concentration increased, fluorescence continued to be quenched and no other metal ions responded significantly, as shown in fig. 6, indicating that it can be used for Hg2+Selective and highly sensitive testing of.
Example 2
The sulfur quantum dots prepared in example 1 were subjected to surface modification treatment. The specific method comprises the following steps:
and (3) adding 100 mu L of hydrazine hydrate into 20mL of sulfur quantum dot solution at room temperature, stirring and reacting for 1h, and performing optical property characterization on the obtained surface-modified sulfur quantum dot to prove that the sulfur quantum dot has the capability of biological imaging.
The modified sulfur quantum dots are used for cell fluorescence imaging, and have high fluorescence quantum yield and good biocompatibility, so that brighter fluorescence signals are displayed in cells.
Example 3
The sulfur quantum dots prepared in example 1 were subjected to surface modification treatment. The specific method comprises the following steps:
at room temperature, 10 μ L of 0.1M glucose oxidase (GOx) was added to 20mL of the sulfur quantum dot solution, and the mixture was stirred for 1 hour to obtain sulfur quantum dots for tumor treatment.
Loaded GOx is able to consume glucose in vivo to produce H2O2To produce the effect of treating hunger.
While the invention has been described with reference to certain preferred embodiments, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention.

Claims (6)

1. A method for rapidly synthesizing strong fluorescent sulfur quantum dots is characterized by comprising the following steps:
step one, adding sulfur powder and metal sulfide into a dispersion system to obtain dispersion liquid; the dispersion system comprises bovine serum albumin and water;
step two, transferring the dispersion liquid into a round-bottom flask, and introducing O3Stirring and reacting under heatingTime;
step three, after the reaction is finished, naturally cooling to room temperature, and carrying out purification treatment through centrifugation, filtration and dialysis to obtain sulfur quantum dots;
wherein the dosage ratio of the sulfur powder, the metal sulfide, the bovine serum albumin and the water is (0.05-1 g): (0.02-0.1 g): (5-10 g): (10-60 mL).
2. The method of claim 1, wherein the sulfur powder comprises one or both of sublimed sulfur powder, elemental sulfur.
3. The method of claim 2, wherein the sulfur powder is sublimed sulfur powder.
4. The method of claim 1, wherein the metal sulfide comprises one or more of sodium sulfide, potassium sulfide, magnesium sulfide, and zinc sulfide.
5. The method of claim 4, wherein the metal sulfide is sodium sulfide.
6. The method as claimed in claim 1, wherein O is introduced3The speed of the reaction is 1-100 mL/min, the heating temperature is 25-150 ℃, the stirring speed is 100-2000 rpm, and the reaction time is 0.1-10 h.
CN202110066431.8A 2021-01-19 2021-01-19 Method for rapidly synthesizing high-fluorescence sulfur quantum dots Active CN112852412B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202110066431.8A CN112852412B (en) 2021-01-19 2021-01-19 Method for rapidly synthesizing high-fluorescence sulfur quantum dots

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202110066431.8A CN112852412B (en) 2021-01-19 2021-01-19 Method for rapidly synthesizing high-fluorescence sulfur quantum dots

Publications (2)

Publication Number Publication Date
CN112852412A CN112852412A (en) 2021-05-28
CN112852412B true CN112852412B (en) 2022-03-29

Family

ID=76007037

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202110066431.8A Active CN112852412B (en) 2021-01-19 2021-01-19 Method for rapidly synthesizing high-fluorescence sulfur quantum dots

Country Status (1)

Country Link
CN (1) CN112852412B (en)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115044368B (en) * 2022-06-22 2023-10-13 成都理工大学 Method for synthesizing sulfur quantum dots by photocatalytic oxidation

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110129040A (en) * 2019-05-08 2019-08-16 桂林理工大学 A kind of preparation method of water soluble fluorescence sulphur quantum dot

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110129040A (en) * 2019-05-08 2019-08-16 桂林理工大学 A kind of preparation method of water soluble fluorescence sulphur quantum dot

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
Two-Step Oxidation Synthesis of Sulfur with a Red Aggregation-;Zhenguang Wang等;《Communications》;20200129;第9997-10002页&附录信息 *
层状硫纳米材料的合成及光电特性研究;白状伟;《中国优秀博硕士学位论文全文数据库（硕士）工程科技Ⅰ辑》;20210115(第1期);第B020-1134页 *

Also Published As

Publication number Publication date
CN112852412A (en) 2021-05-28

Similar Documents

Publication Publication Date Title
Liu et al. Carbon dots: synthesis, formation mechanism, fluorescence origin and sensing applications
CN110734763B (en) Sulfur quantum dot and preparation method and application thereof
Shi et al. Fluorescent carbon dots for bioimaging and biosensing applications
CN106566534A (en) Red-light carbon dot of high yield and high quantum yield, and preparation method thereof
CN110272734B (en) Preparation method and application of high-quantum-yield carbon quantum dots for NO detection
US11407941B2 (en) Fluorescent nanomaterial and preparation method and applications thereof
Qiao et al. Rapid conversion from common precursors to carbon dots in large scale: Spectral controls, optical sensing, cellular imaging and LEDs application
Zhu et al. Blue-emitting carbon quantum dots: Ultrafast microwave synthesis, purification and strong fluorescence in organic solvents
Shao et al. A reformative oxidation strategy using high concentration nitric acid for enhancing the emission performance of graphene quantum dots
CN112852412B (en) Method for rapidly synthesizing high-fluorescence sulfur quantum dots
JP2014185224A (en) Semiconductor nanoparticle and fluorescent probe for labeling biological samples
CN108516533A (en) A kind of preparation method of hair peak green fluorescent carbon point
CN107603612B (en) Preparation method and application of hollow orange fluorescent carbon nanoparticles
CN109796974B (en) Preparation method of graphene quantum dots with adjustable fluorescence properties
CN101724402A (en) Preparation method of CdSe/SiO2 quantum dot composite fluorescent nanoparticles
CN107325815A (en) High quantum production rate fluorescent carbon point of N doping and its preparation method and application
CN111518552B (en) Preparation of fluorine-containing graphene quantum dots and application of fluorine-containing graphene quantum dots as photodynamic therapy photosensitizer
CN107603608B (en) Method for preparing fluorescent carbon dots by taking gynostemma pentaphylla as carbon source
CN111088034A (en) Lead-free bismuth-based perovskite @ SiO2Core-shell material and preparation method and application thereof
CN111073638A (en) Method for preparing controllable photoluminescence carbon dots by changing temperature
CN114958364A (en) Preparation method and application of green fluorescent graphene quantum dots
CN107804840B (en) The method that hydro-thermal cutting high yield prepares coal base graphene quantum dot
CN113460995A (en) Method for simultaneously preparing carbon dots and nano zinc oxide
CN112268882B (en) Preparation method and application of carbon dot-manganese dioxide nano fluorescent probe for high-selectivity detection of glutathione
CN109456755B (en) Method for preparing silicon dioxide particles containing methylene blue and having high fluorescence intensity by hydrothermal method

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant